JP4200107B2 - Method for analyzing impurities in silicon - Google Patents
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- JP4200107B2 JP4200107B2 JP2004004529A JP2004004529A JP4200107B2 JP 4200107 B2 JP4200107 B2 JP 4200107B2 JP 2004004529 A JP2004004529 A JP 2004004529A JP 2004004529 A JP2004004529 A JP 2004004529A JP 4200107 B2 JP4200107 B2 JP 4200107B2
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- 229910052710 silicon Inorganic materials 0.000 title claims description 39
- 239000010703 silicon Substances 0.000 title claims description 39
- 238000000034 method Methods 0.000 title claims description 31
- 239000012535 impurity Substances 0.000 title claims description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 31
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 21
- 229910017604 nitric acid Inorganic materials 0.000 claims description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000004090 dissolution Methods 0.000 claims description 20
- 238000004458 analytical method Methods 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000009616 inductively coupled plasma Methods 0.000 claims description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 10
- 229910052796 boron Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004993 emission spectroscopy Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Sampling And Sample Adjustment (AREA)
Description
本発明は、シリコン、特に、冶金級シリコン中に存在するホウ素等の不純物を定量するための分析方法に関する。詳しくは、シリコン中の上記不純物を高精度で定量することが可能な分析方法を提供するものである。 The present invention relates to an analytical method for quantifying impurities such as boron present in silicon, particularly metallurgical grade silicon. Specifically, the present invention provides an analysis method capable of quantifying the impurities in silicon with high accuracy.
高純度シラン合成プロセスにおいては、原料として使用量の多い冶金級シリコン中の不純物量をコントロールすることが求められている。そのために、不純物量を正確に定量する分析手段が必要となっている。 In a high-purity silane synthesis process, it is required to control the amount of impurities in metallurgical grade silicon that is used in large quantities as a raw material. For this purpose, an analysis means for accurately quantifying the amount of impurities is required.
従来、シリコンウエハーにおける不純物の分析に対して要求される精度が比較的低い冶金級シリコン等のシリコン中の不純物の分析は、誘導結合プラズマ発光分光分析（ＩＣＰ−ＡＥＳ）等の誘導結合プラズマ発光分析（ＩＣＰ）で正確に行なうことが可能である。 Conventionally, the analysis of impurities in silicon, such as metallurgical grade silicon, which is relatively low in accuracy required for the analysis of impurities in silicon wafers, is performed by inductively coupled plasma emission spectrometry (ICP-AES) or the like. (ICP) can be performed accurately.
上記方法において、シリコン及び不純物は溶液として分析装置に供給する必要がある。従来、シリコンを溶解するには、硝酸及びフッ酸の水溶液中で加熱溶解する方法が知られており、かかる操作によって得られた溶解液を純水により適当な希釈倍率に調製してＩＣＰの分析装置に供給する方法が考えられる。 In the above method, silicon and impurities need to be supplied to the analyzer as a solution. Conventionally, in order to dissolve silicon, a method of dissolving by heating in an aqueous solution of nitric acid and hydrofluoric acid is known, and an ICP analysis is performed by preparing a solution obtained by such an operation with pure water to an appropriate dilution ratio. A method of supplying the apparatus is conceivable.
しかしながら、上記方法はＩＣＰによる不純物、特に、ホウ素の定量精度が十分ではなく、更に改良の余地があった。 However, the above-mentioned method has not enough accuracy for determination of impurities by ICP, particularly boron, and there is room for further improvement.
従って、本発明の目的は、ＩＣＰによるシリコン中の不純物の分析において、その精度を改良した定量分析方法を提供することにある。 Accordingly, an object of the present invention is to provide a quantitative analysis method with improved accuracy in the analysis of impurities in silicon by ICP.
本発明者は、上記技術課題を解決すべく鋭意研究を行ってきた。その結果、溶解に使用する硝酸が、ＩＣＰ、特に、ＩＣＰ−ＡＥＳによる分析において測定対象となる不純物の回収率を低下する影響を及ぼすという知見を得た。そして、上記知見に基づき、シリコンの溶解液より硝酸を除去し、これを塩酸水溶液に再溶解したものをＩＣＰに供したところ、その測定感度を低下させることなく、前記回収率を飛躍的に向上せしめることができ、かかる分析における定量精度が極めて効果的に向上し得ることを見出し、本発明を完成するに至った。 The inventor has conducted intensive research to solve the above technical problems. As a result, it was found that nitric acid used for dissolution has an effect of reducing the recovery rate of impurities to be measured in the analysis by ICP, particularly ICP-AES. And based on the above knowledge, nitric acid was removed from the silicon solution, and this was redissolved in an aqueous hydrochloric acid solution and subjected to ICP. The recovery rate was dramatically improved without reducing the measurement sensitivity. As a result, the inventors have found that the quantitative accuracy in such analysis can be improved extremely effectively, and have completed the present invention.
即ち、本発明は、硝酸及びフッ酸の水溶液中でシリコンよりなる試料を溶解してシリコン溶解液を得る溶解工程、上記溶解工程によって得られたシリコン溶解液を１００〜１６０℃の温度に加熱することにより濃縮して硝酸が除去された濃縮液を得る濃縮工程、上記濃縮工程より得られた濃縮液を塩酸水溶液に溶解する再溶解工程、及び、再溶解工程より得られる再溶解液を誘導結合プラズマ発光分析により分析することにより該再溶解液に含有されている不純物を定量する定量工程より成ることを特徴とするシリコン中のホウ素の分析方法である。
That is, the present invention dissolves a sample made of silicon in an aqueous solution of nitric acid and hydrofluoric acid to obtain a silicon solution, and heats the silicon solution obtained by the dissolution step to a temperature of 100 to 160 ° C. Concentration step to obtain a concentrate from which nitric acid has been removed by concentration, a re-dissolution step for dissolving the concentrate obtained from the concentration step in an aqueous hydrochloric acid solution, and a re-dissolution solution obtained from the re-dissolution step inductively coupled It is a method for analyzing boron in silicon, characterized by comprising a quantitative step of quantifying impurities contained in the redissolved solution by analysis by plasma emission analysis.
本発明の分析方法は、簡易な操作によってシリコン中の不純物元素の定量を高い精度で行なうことが可能である。特に、不純物として含有されるホウ素の回収率は９２〜９５％或いはそれ以上に達し、シリコン中のホウ素の定量方法として高く評価することができる。 The analysis method of the present invention can determine the impurity element in silicon with high accuracy by a simple operation. In particular, the recovery rate of boron contained as impurities reaches 92 to 95% or more, and can be highly evaluated as a method for quantifying boron in silicon.
本発明において、分析の対象となるシリコンは特に制限されないが、高純度シラン製造プロセスにおいて使用される冶金級シリコン中を対象とし、その不純物の測定に対して好適である。上記冶金級シリコンは、珪石を還元して作られるものであり、約９０〜９９．９重量％の純度を有するシリコンである。 In the present invention, the silicon to be analyzed is not particularly limited, but is suitable for the measurement of impurities in metallurgical grade silicon used in a high purity silane production process. The metallurgical grade silicon is made by reducing silica and has a purity of about 90 to 99.9% by weight.
本発明において、シリコンは、分析に際して、適当な粒径に粉砕することが好ましい。一般には、１０〜２０００μｍの大きさが好ましい。 In the present invention, silicon is preferably pulverized to an appropriate particle size for analysis. In general, a size of 10 to 2000 μm is preferable.
本発明のシリコン中の不純物の分析方法は、（１）溶解工程、（２）濃縮工程、（３）再溶解工程、及び（４）定量工程より成る。 The method for analyzing impurities in silicon according to the present invention comprises (1) a dissolution step, (2) a concentration step, (3) a redissolution step, and (4) a quantitative step.
（１）溶解工程
本発明において、溶解工程は、硝酸及びフッ酸の水溶液中でシリコンよりなる試料を溶解してシリコン溶解液を得る工程である。
(1) Dissolution Step In the present invention, the dissolution step is a step of obtaining a silicon solution by dissolving a sample made of silicon in an aqueous solution of nitric acid and hydrofluoric acid.
上記シリコンの溶解の条件は、硝酸及びフッ酸の水溶液を使用する方法であれば、公知の条件が特に制限なく採用される。好ましい方法を例示すれば、シリコンの粉砕物中に硝酸水溶液を投入後、これにフッ酸水溶液を徐々に添加する方法が好適である。この場合、得られるシリコン溶解液の温度上昇による不純物の揮散を防止するために、硝酸水溶液の使用量を増やすことによって徐熱を効率よく行なうようにする方法、硝酸水溶液を氷冷することによって徐熱を行なう方法などが挙げられる。 The conditions for dissolving the silicon are not particularly limited as long as they are a method using an aqueous solution of nitric acid and hydrofluoric acid. For example, a preferable method is to add an aqueous nitric acid solution to a pulverized silicon and then gradually add an aqueous hydrofluoric acid solution thereto. In this case, in order to prevent the volatilization of impurities due to the temperature rise of the silicon solution to be obtained, a method of efficiently performing slow heating by increasing the amount of nitric acid aqueous solution used, or by gradually cooling the nitric acid aqueous solution with ice cooling. The method of performing heat etc. are mentioned.
上記方法によって、溶解時の液温度を４０℃以下、１０〜４０℃に調節することが好ましい。 It is preferable to adjust the liquid temperature at the time of dissolution to 40 ° C. or lower and 10 to 40 ° C. by the above method.
また、上記硝酸水溶液の濃度は特に制限されないが、３０〜７０重量％程度が好ましい。一方、フッ酸水溶液の濃度は、３０〜５０重量％程度が好ましい。 The concentration of the aqueous nitric acid solution is not particularly limited, but is preferably about 30 to 70% by weight. On the other hand, the concentration of the hydrofluoric acid aqueous solution is preferably about 30 to 50% by weight.
尚、これら硝酸水溶液、フッ酸水溶液は、不純物が極力除去されたものを使用することが好ましく、測定対象とする不純物の濃度がそれぞれ１００ｐｐｔ以下であることが好ましい。 The nitric acid aqueous solution and hydrofluoric acid aqueous solution are preferably those from which impurities are removed as much as possible, and the concentration of the impurity to be measured is preferably 100 ppt or less.
また、溶解に使用する容器は、ポリ四フッ化エチレン等のフッ素樹脂製のものが好適である。 The container used for dissolution is preferably made of a fluororesin such as polytetrafluoroethylene.
（２）濃縮工程
本発明において、濃縮工程は、上記溶解工程によって得られたシリコン溶解液を濃縮して硝酸が除去された濃縮液を得る工程である。
(2) Concentration process In this invention, a concentration process is a process of concentrating the silicon solution obtained by the said melt | dissolution process, and obtaining the concentrate from which nitric acid was removed.
従って、濃縮によって硝酸の殆どが除去される条件が特に制限なく採用される。好適な条件を例示すれば、ホットプレートの如き加熱器を使用し、シリコン溶解液を入れた容器を、１００〜１６０℃で２〜５時間加熱する方法が好適である。
Therefore, the conditions under which most of the nitric acid is removed by concentration are employed without any particular limitation. As an example of suitable conditions, a method of heating a container containing a silicon solution at 100 to 160 ° C. for 2 to 5 hours using a heater such as a hot plate is preferable.
硝酸は、完全に除去することが好ましいが、本発明においては、１重量％程度まで、許容することができる。 Nitric acid is preferably completely removed, but in the present invention, it can be tolerated up to about 1% by weight.
尚、フッ酸は反応によって殆ど消失するが、過剰に使用した場合は、これも除去することが好ましい。一般に、フッ酸は、上記硝酸の除去条件において同時に除去される。 Although hydrofluoric acid almost disappears due to the reaction, it is preferably removed when used in excess. In general, hydrofluoric acid is simultaneously removed under the above-mentioned nitric acid removal conditions.
（３）再溶解工程
本発明において、再溶解工程は、上記濃縮工程より得られた、硝酸を除去された濃縮液を塩酸水溶液に溶解する工程である。
(3) Re-dissolution process In this invention, a re-dissolution process is a process of melt | dissolving the concentrated liquid obtained from the said concentration process from which the nitric acid was removed in hydrochloric acid aqueous solution.
かかる濃縮液は、硝酸等の除去により、一部固体の析出が起こる場合が多く、該固体を溶解してＩＣＰによる分析を可能とする必要がある。 In such a concentrated liquid, precipitation of a part of solid often occurs due to removal of nitric acid or the like, and it is necessary to dissolve the solid to enable analysis by ICP.
本発明においては、上記析出した固体の再溶解に塩酸水溶液を使用することを特徴とする。即ち、塩酸水溶液の使用により、分析感度を低下させることなく、ＩＣＰにおける回収率を上げることができる。 In the present invention, an aqueous hydrochloric acid solution is used for redissolving the precipitated solid. That is, by using an aqueous hydrochloric acid solution, the recovery rate in ICP can be increased without lowering the analytical sensitivity.
上記塩酸水溶液の濃度は、５〜３５重量％程度が好ましい。 The concentration of the hydrochloric acid aqueous solution is preferably about 5 to 35% by weight.
尚、この塩酸水溶液は、不純物が極力除去されたものを使用することが好ましく、測定対象とする不純物の濃度が１００ｐｐｔ以下であることが好ましい。 In addition, it is preferable to use this hydrochloric acid aqueous solution from which impurities are removed as much as possible, and it is preferable that the concentration of impurities to be measured is 100 ppt or less.
また、上記方法によって得られた再溶解液は、必要に応じて純水で適当な濃度に希釈して、再溶解液として続く定量工程に供することができる。 Moreover, the redissolved solution obtained by the above method can be diluted to an appropriate concentration with pure water as necessary, and used as a redissolved solution for the subsequent quantitative step.
更に、ＩＣＰ−ＡＥＳの分析装置におけるトラブルを防止するため、上記再溶解液は、ろ過してパーティクルを除去する操作を行うことが好ましい。 Furthermore, in order to prevent troubles in the ICP-AES analyzer, the re-dissolved solution is preferably filtered to remove particles.
（４）定量工程
本発明において、定量工程は、上記再溶解工程より得られる再溶解液をＩＣＰにより分析することにより該再溶解液に含有されている不純物を定量する工程である。
(4) Quantification process In this invention, a quantification process is a process of quantifying the impurity contained in this re-dissolution liquid by analyzing the re-dissolution liquid obtained from the said re-dissolution process by ICP.
ＩＣＰによる分析は、公知の装置を使用して公知の方法によって行なうことができる。具体的には、ＩＣＰ−ＡＥＳ、ＩＣＰ−ＭＳ等を挙げることができるが、本発明においては、ＩＣＰ−ＡＥＳによる分析方法が特に好ましい。 Analysis by ICP can be performed by a known method using a known apparatus. Specific examples include ICP-AES and ICP-MS. In the present invention, an analysis method using ICP-AES is particularly preferable.
本発明を更に具体的に説明するため以下実施例を挙げて説明するが、本発明はこれらの実施例に限定されるものではない。 The present invention will be described more specifically with reference to the following examples. However, the present invention is not limited to these examples.
実施例１
５０ｍｌのテフロン（登録商標）製ビーカーに冶金級シリコン試料を０．５ｇ〜１．０ｇ精秤した。その中に７Ｎ−ＨＮＯ３３０ｍｌを加えた。さらに、ＨＦ（５０重量％）を徐々に加えて試料を分解した。それをホットプレート上に乗せ、温度１４０℃で２時間加熱させた後、ホットプレート温度１６０℃で１時間、さらにホットプレート温度１４０℃に調整し、残液が少量になるまで加熱した。その中に、回収試薬として、ＨＣｌ（３５重量％）を２ｍｌ添加し、さらに純水５ｍｌを加え、ホットプレート温度１４０℃で５分間加熱した。ビーカーをホットプレートから降ろし、常温まで冷ました。ビーカー内の試料液をポリエチレン製漏斗とろ紙を用いて、ポリエチレン製１００ｍｌメスフラスコにろ過し、さらに純水にて、１００ｍｌまでメスアップした。
Example 1
A metallurgical grade silicon sample was accurately weighed in a 50 ml Teflon (registered trademark) beaker. Into this, 30 ml of 7N-HNO 3 was added. Further, HF (50% by weight) was gradually added to decompose the sample. It was placed on a hot plate and heated at a temperature of 140 ° C. for 2 hours, then adjusted to a hot plate temperature of 160 ° C. for 1 hour and further to a hot plate temperature of 140 ° C., and heated until the residual liquid became small. 2 ml of HCl (35% by weight) was added as a recovery reagent, 5 ml of pure water was further added, and heated at a hot plate temperature of 140 ° C. for 5 minutes. The beaker was removed from the hot plate and cooled to room temperature. The sample solution in the beaker was filtered into a polyethylene 100 ml volumetric flask using a polyethylene funnel and filter paper, and further made up to 100 ml with pure water.
この液をＩＣＰ−ＡＥＳ装置として２波シーケンシャル形プラズマ発光分析装置 ＩＣＰＳ−１０００Ｖ形（株式会社島津製作所社製）に導入して分析した結果、ホウ素の検出下限は１０ｐｐｂであり、高感度で分析できた。この時のホウ素の回収率は９２％であった。 As a result of introducing this solution into an ICPS-1000V type ICPS-1000V type (manufactured by Shimadzu Corporation) as an ICP-AES device and analyzing it, the lower limit of detection of boron is 10 ppb, which can be analyzed with high sensitivity. It was. The boron recovery rate at this time was 92%.
比較例
５０ｍｌのテフロン（登録商標）製ビーカーに冶金級シリコン試料を０．５ｇ〜１．０ｇ精秤した。その中に７Ｎ−ＨＮＯ３５ｍｌを加えた。これを冷水中に浸け、さらに、ＨＦ（５０重量％）を徐々に加えて試料を分解した。それをウォーターバス中にて温度６０℃で２〜３時間加熱させた後、ビーカーをウォーターバスから降ろし、常温まで冷ました。ビーカー内の試料液をポリエチレン製漏斗とろ紙を用いて、ポリエチレン製５０ｍｌメスフラスコにろ過し、さらに純水にて、５０ｍｌまでメスアップした。
Comparative Example A metallurgical grade silicon sample was precisely weighed in a 50 ml Teflon (registered trademark) beaker. It was added 7N-HNO 3 5 ml therein. This was immersed in cold water, and HF (50% by weight) was gradually added to decompose the sample. After heating it in a water bath at a temperature of 60 ° C. for 2-3 hours, the beaker was removed from the water bath and cooled to room temperature. The sample solution in the beaker was filtered into a polyethylene 50 ml volumetric flask using a polyethylene funnel and filter paper, and further diluted to 50 ml with pure water.
この液をＩＣＰ−ＡＥＳ装置として２波シーケンシャル形プラズマ発光分析装置 ＩＣＰＳ−１０００Ｖ形（株式会社島津製作所社製）に導入して分析した結果、ホウ素の検出下限は１００ｐｐｂであった。また、この時のホウ素の回収率は５５％であった。
As a result of introducing this solution into a two-wave sequential plasma emission analyzer ICPS-1000V type (manufactured by Shimadzu Corporation) as an ICP-AES apparatus, the lower limit of detection of boron was 100 ppb. Further, the recovery rate of boron at this time was 55%.
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| JP2004004529A JP4200107B2 (en) | 2004-01-09 | 2004-01-09 | Method for analyzing impurities in silicon |
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| JP4200107B2 true JP4200107B2 (en) | 2008-12-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102590183A (en) * | 2012-03-06 | 2012-07-18 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method capable of quantitatively screening substance of very high concern in rubber and plastic products using microwave digestion-ICP-AES method |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4800806B2 (en) * | 2006-03-23 | 2011-10-26 | 日本碍子株式会社 | Method for preparing sample solution for impurity analysis in silicon compound-containing sample |
| JP5131245B2 (en) * | 2009-05-21 | 2013-01-30 | 株式会社Ｓｕｍｃｏ | Method for analyzing metal impurities in silicon powder |
| JP6329920B2 (en) * | 2015-04-14 | 2018-05-23 | 信越化学工業株式会社 | Method for evaluating polycrystalline silicon mass |
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- 2004-01-09 JP JP2004004529A patent/JP4200107B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590183A (en) * | 2012-03-06 | 2012-07-18 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method capable of quantitatively screening substance of very high concern in rubber and plastic products using microwave digestion-ICP-AES method |
| CN102590183B (en) * | 2012-03-06 | 2014-01-08 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method capable of quantitatively screening substance of very high concern in rubber and plastic products using microwave digestion-ICP-AES method |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
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